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Zhang H.-W.,Shandong Marine Resource and Environment Research Institute | Zhang H.-W.,Yantai Shanshui Seafood Co. | Liu H.-H.,Shandong Marine Resource and Environment Research Institute | Liu H.-H.,Shandong Province Key Laboratory of Restoration for Marine Ecology | And 12 more authors.
Journal of Chinese Mass Spectrometry Society | Year: 2015

A method for determination of 9 triazine herbicides residues in aquatic products by gel permeation chromatography-solid phase extraction-gas chromatography tandem mass spectrometry(GPC-SPE-GC-MS/MS) was established. The sample was extracted with ethyl acetate, then cleaned up by gel permeation chromatography and purified by carbon and NH2 solid phase extraction column. The analytes were determined in selected ion monitoring and quantified by external method. Propazine, atrazine, terbuthylazine, simazine and cyprazine show good linearity in the range of 1.0-50.0 μg/L, and the detection limits of the five analytes are 1.0 μg/kg. The average recoveries range from 86.3% to 119% when spiked at 1.0-10.0 μg/kg with relative standard deviations from 5.11% to 10.1%. Simetryn, prometryn, ametryn and terbutryn show good linearity in the range of 2.0-100.0 μg/L, and the detection limits are 2.0 μg/kg. The average recoveries range from 87.6% to 112% when spiked at 2.0-20.0 μg/kg with relative standard deviations from 5.27% to 9.56%. The method is stable and reasonable, and which can be used for the determination of 9 triazine herbicides residues in aquatic products. ©, 2015, Chinese Society for Mass Spectrometry. All right reserved.


Xu Y.-J.,Marine Fisheries Research Institute of Shandong Province | Xu Y.-J.,Shandong Province Key Laboratory of Restoration for Marine Ecology | Tian X.-H.,Marine Fisheries Research Institute of Shandong Province | Tian X.-H.,Shandong Province Key Laboratory of Restoration for Marine Ecology | And 11 more authors.
Journal of Chromatographic Science | Year: 2012

This work describes solid-phase extraction-ultra-performance liquid chromatography with electrospray ionization tandem spectrometry for determination of malachite green and metabolite leucomalachite green, crystal violet and metabolite leucocrystal violet, methylene blue and metabolites including azure A, azure B and azure C in aquatic products. Samples were extracted with acetonitrile and ammonium acetate buffer and purified by liquid extraction with dichloromethane, and then on MCAX solid-phase extraction cartridges. Then the extract was evaporated at 458C by nitrogen blow. The residue was dissolved and separated by an Acquity BEH C18 column. The mobile phase was acetonitrile (A) and 5 mmol/L of ammonium acetate containing 0.1% formic acid (B). Analytes were confirmed and quantified using a tandem mass spectrometry system in multiple reaction mode with triple quadrupole analyzer using positive polarity mode. The limits of detection of malachite green, leucomalachite green, crystal violet and leucocrystal violet were 0.15 μg/kg, the limits of quantification were 0.50 μg/kg, and the average recoveries were more than 75% with spiked residues from 0.5 to 10 μg/kg. The relative standard deviations were less than 13%. The limits of detection of methylene blue, azure A, azure B and azure C were 0.3 μg/kg, the limits of quantification were 1.0 μg/kg, the average recoveries were more than 70% with spiked residues from 1.0 to 10 μg/kg and the relative standard deviations were less than 15%. The method has the merits of simplicity, sensitivity and rapidity, and can be used for simultaneous determination of the analytes in aquatic products. © The Author [2012]. Published by Oxford University Press. All rights reserved.


Xu Y.,Marine Fisheries Research Institute of Shandong Province | Xu Y.,Shandong Province Key Laboratory of Restoration for Marine Ecology | Tian X.,Marine Fisheries Research Institute of Shandong Province | Tian X.,Shandong Province Key Laboratory of Restoration for Marine Ecology | And 11 more authors.
Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences | Year: 2012

A rapid and simple method for the determination of colistin A and B in fishery products by reversed phase ultra performance liquid chromatography with positive electrospray ionization tandem spectrometry (UPLC-ESI-MS/MS) method was described. The samples were extracted with 1.0mol/L of hydrochloric acid in methanol-water and then purified on the PLS solid phase extraction columns. Then the eluate was evaporated to less than 1mL under a gentle stream of nitrogen at 40°C and formic acid-acetonitrile-water (0.2/10/90, v/v/v) was added to adjust volume to 1mL final volume. An aliquot (10μL) was injected onto the LC column for analysis with the mobile phase of 0.2% formic acid in acetonitrile and 0.2% formic acid in water at 0.20mLmin -1. Multiple reaction monitoring was performed using precursor-product ion combinations. Calibration curves were linear from 200ng/mL to 2000ng/mL for colistin A and B. Mean recoveries were between 72.9% and 82.9%. The LOD was 10.0μg/kg and LOQ was 40.0μg/kg. The intra-day assay precision values for QC samples were between 2.17% and 9.00%, and inter-day values were between 2.80% and 6.97%. The method has merits of simplicity, sensitivity and rapidity, and it can be used for the determination of colistin A and B in fishery products. © 2012.


Ren C.-B.,Marine Fisheries Research Institute of Shandong Province | Ren C.-B.,Yantai Shanshui Seafood Co. | Tian X.-H.,Marine Fisheries Research Institute of Shandong Province | Tian X.-H.,Shandong Province Key Laboratory of Restoration for Marine Ecology | And 10 more authors.
Journal of Chinese Mass Spectrometry Society | Year: 2013

The triazine herbicides in seawater were determined by solid phase extraction ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry(UPLC-ESI-MS/MS). UPLC and MS/MS analytical conditions were examined and optimized critically by a series of experiments. Samples were filtrated and purified on the HLB solid phase extraction cartridges. The elution was collected and evaporated to less than 1 mL at 40°C by nitrogen blow, then added to 1 mL acetonitrile and water (1:1, V/V) and ultrasonic wave extraction for 1 min. After filtrated with 0.22 μm filter membrane, the residue was separated by Acquity™ UPLC HSS C18 column (2.1 mm×100 mm×1.8 μm) using gradient elution separation. The mobile phase was a mixture of A (acetonitrile) and B (5 mmol/L ammonium acetate containing 0.1% formic acid) in a flow rate of 0.25 mL/min. Finally analytes were confirmed and quantified using MS/MS system in multiple reaction mode with triple quadrapole analyzer using positive polarity mode. The analytes show good linearity in the range of 1 ng/L to 50 ng/L with correlation coefficient from 0.992 to 0.999. The detection limit is 1 ng/L, and quantification limit is 2 ng/L. The average recoveries at three dose levels(2 ng/L, 5 ng/L and 10 ng/L) are 65.8%-103% with relative standard deviations from 4.84% to 15.2%. In addition, the method has merits of simplicity, sensitivity and rapidity, and can be used for simultaneous determination of triazine herbicides in seawater.

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